高效液相色谱串联质谱法测定水产养殖水中氟虫腈及其代谢物残留

    Determination of Fipronil and Its Metabolite Residues in the Aquaculture Water by High-performance Liquid Chromatography-tandem Mass Spectrometry

    • 摘要: 为了能够快速筛查水产养殖水中氟虫腈及其代谢物含量,使用液液萃取前处理,高效液相色谱-串联质谱联用建立了养殖水中氟虫腈及其代谢物的检测方法。优化后的前处理条件:养殖水过滤后取100.0 mL,以石油醚作为萃取溶剂,摇匀后,取上清液,共提取3次,提取液40℃以下氮吹近干,以1.0 mL甲醇水复溶,过膜,上机检测。色谱条件:色谱柱:Eclipse Plus C18,流动相为甲醇-水,在7 min内氟虫腈及其代谢物分离良好。质谱条件:电喷雾离子源(ESI);负离子模式同时扫描;多反应监测(MRM)采集方式。氟虫腈及其代谢物在10~500 ng·mL-1的范围内均具有良好的线性关系,相关系数不小于0.999,平均加标回收率为65.9%~88.5%,相对标准偏差为1.8%~13%,各组分方法定量限为0.1 ng·mL-1时信噪比均大于10。该方法适用于养殖水中氟虫腈及其代谢物的快速检测。

       

      Abstract: In order to quickly screen the content of fipronil and its metabolites in the aquaculture water, a method for the detection of fipronil and its metabolites in the aquaculture water was established by using the liquid-liquid extraction pretreatment and the high-performance liquid chromatography-tandem mass spectrometry. The optimized pretreatment conditions were as follows:100.0 mL aquaculture water was selected after the filtration, and the petroleum ether was used as the extraction solvent. After shaking well, the supernatant was taken and extracted for 3 times. The extracting solution was dried by nitrogen below 40℃, redissolved with 1.0 mL methanol water, passed through the membrane, and detected on the machine. The chromatographic conditions were as follows:the chromatographic column was Eclipse Plus C18, the mobile phase was methanol-water, and the fipronil and its metabolites were well separated within 7 min. The mass spectrometry conditions were as follows:the electrospray ionization source (ESI); simultaneously scanning by using the negative ion mode; the acquisition mode with the multiple reaction monitoring (MRM). Fipronil and its metabolites had a good linear relationship in the range of 10 ng·mL-1-500 ng·mL-1, the correlation coefficient was not less than 0.999, the average recovery rate was 65.9%-88.5%, and the relative standard deviation was 1.8%-13%. The signal-to-noise ratio (SNR) was all greater than 10 when the limit of quantification of each component method was 0.1 ng·mL-1. The method was suitable for the rapid detection of fipronil and its metabolites in the aquaculture water.

       

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